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WO2022056351A1 - Systèmes et procédés pour déterminer la teneur en eau d'un échantillon - Google Patents

Systèmes et procédés pour déterminer la teneur en eau d'un échantillon Download PDF

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Publication number
WO2022056351A1
WO2022056351A1 PCT/US2021/050000 US2021050000W WO2022056351A1 WO 2022056351 A1 WO2022056351 A1 WO 2022056351A1 US 2021050000 W US2021050000 W US 2021050000W WO 2022056351 A1 WO2022056351 A1 WO 2022056351A1
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WO
WIPO (PCT)
Prior art keywords
membrane
sample
water
absorbance
oil
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US2021/050000
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English (en)
Inventor
Sfoog H. SALEH
Carl P. Tripp
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Maine System
Original Assignee
University of Maine System
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Filing date
Publication date
Application filed by University of Maine System filed Critical University of Maine System
Priority to CA3194337A priority Critical patent/CA3194337A1/fr
Priority to EP21867736.7A priority patent/EP4211446A4/fr
Priority to US18/025,938 priority patent/US20230366814A1/en
Publication of WO2022056351A1 publication Critical patent/WO2022056351A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3554—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for determining moisture content
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N22/00—Investigating or analysing materials by the use of microwaves or radio waves, i.e. electromagnetic waves with a wavelength of one millimetre or more
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26—Oils; Viscous liquids; Paints; Inks
    • G01N33/28—Oils, i.e. hydrocarbon liquids
    • G01N33/2835—Specific substances contained in the oils or fuels
    • G01N33/2847—Water in oils
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/405—Concentrating samples by adsorption or absorption
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
    • G01N2021/3155—Measuring in two spectral ranges, e.g. UV and visible
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light

Definitions

  • the present disclosure is directed to methods of measuring water concentration in a sample including steps of passing a sample through a membrane that is transparent to one or more forms of radiation in at least one region of interest, irradiating the membrane with the one or more forms of radiation, and determining water concentration in the sample from one or more absorbance and/or Raman peaks.
  • one or more forms of radiation applied to a sample in a method described herein includes microwave, infrared, visible, and/or ultraviolet light.
  • one or more forms of radiation applied to a sample in a method described herein includes infrared light.
  • a determining step of a method provided herein includes a step of measuring reflected, transmitted, emitted and/or scattered light.
  • a membrane in a method described herein, is cooled and/or purged with a gas that is substantially free of water prior to a step of passing a sample through the membrane.
  • a membrane in a method described herein, is cooled under vacuum prior to the step of passing a sample through the membrane.
  • a membrane is cooled for at least a portion of the passing, irradiating, and determining steps of the method.
  • a membrane in a method described herein, is cooled to a temperature between -196 °C to 10 °C, inclusive.
  • one or more absorbance and/or Raman peaks measured in a method described herein are characterized in that they occur at a wavelength selected from the group consisting of about 5185 cm -1 , about 3420 cm -1 , about 2127 cm -1 , about 1650 cm -1 , about 800 cm -1 and combinations thereof.
  • water concentration in a sample analyzed by a method described herein is in a range of about 1 ppm to about 10,000 ppm.
  • water concentration in a sample analyzed by a method described herein is in a range of about 1 ppm to about 1,000 ppm.
  • water concentration in a sample analyzed by a method described herein is in a range of about 1,000 ppm to about 10,000 ppm.
  • one or more absorbance and/or Raman peaks measured in a method described herein are characterized by a wavelength of about 3420 cm -1 .
  • one or more absorbance and/or Raman peaks measured in a method described herein are characterized by a wavelength of about 2127 cm -1 .
  • the present disclosure is directed to methods of measuring water concentration in a sample including steps of adding an agent to a sample to react with and/or adsorb water from the sample, thereby forming a solid particulate material, collecting the solid particulate material on a membrane that is transparent to one or more forms of radiation in at least one region of interest, irradiating the membrane with the one or more forms of radiation, and determining water concentration in the sample from one or more absorbance and/or Raman peaks.
  • one or more forms of radiation includes microwave, infrared, visible, or ultraviolet light.
  • one or more forms of radiation includes infrared light.
  • a determining step of a method described herein includes a step of measuring reflected, transmitted, emitted or scattered light.
  • a step of adding an agent to a sample includes adding a membrane coated in an agent to the sample.
  • an agent added to a sample in a method described herein is selected from the group consisting of calcium oxide, magnesium oxide, copper sulfate, zinc oxide, sodium oxide, iron chloride, cobalt nitrate, nickel sulfate, tungsten oxide, alumina, silica, titania, calcium hydride, and combinations thereof.
  • an agent added to a sample in a method described herein is calcium oxide.
  • the calcium oxide reacts with water to form Ca(OH) 2 .
  • an agent added to a sample in a method described herein is copper sulfate.
  • copper sulfate is added as an agent to a sample in a method described herein, the copper sulfate adsorbs water to form a hydrate.
  • one or more absorbance and/or Raman peaks measured are characterized by a wavelength in a range of about 3500 cm -1 to about 3100 cm -1 , in a range of about 1600 cm -1 to about 1800 cm -1 , or combinations thereof.
  • one or more absorbance and/or Raman peaks measured in a method described herein are characterized by a wavelength of about 3420 cm -1 , 3190 cm -1 , 1743 cm -1 , 1667 cm -1 , or combinations thereof.
  • the hydrate comprises copper sulfate monohydrate.
  • one or more absorbance and/or Raman peaks measured are characterized by a wavelength of about 3190 cm -1 , about 1743 cm -1 , or combinations thereof.
  • one or more absorbance and/or Raman peaks measured are characterized by a wavelength of about 1743 cm -1 .
  • water concentration in a sample is in a range of about 1 ppm to about 10,000 ppm.
  • an amount of an agent is added to a sample such that absence of an absorbance peak at 3420 cm -1 indicates complete consumption of water in a sample.
  • a sample is an oil.
  • a membrane is at least partially coated in oil.
  • an oil that is at least partially coating a membrane is a secondary oil.
  • a membrane has a diameter of 1 to 80 mm.
  • a membrane has a diameter of 10 to 50 mm.
  • one or more absorbance and/or Raman peaks measured in a method described herein are measured with a Fourier Transform Infrared Spectrometer (FTIR), a dispersive infrared both single and double beam, a filtermetric spectrometer, a tunable laser based infrared spectrometer, or a Raman spectrometer.
  • FTIR Fourier Transform Infrared Spectrometer
  • the present disclosure is directed to kits for measuring water concentration in a sample including one or more doses of an agent and a membrane assembly containing a membrane.
  • an agent of a kit is selected from calcium oxide, magnesium oxide, copper sulfate, zinc oxide, sodium oxide, iron chloride, cobalt nitrate, nickel sulfate, tungsten oxide, alumina, silica, titania, calcium hydride, and combinations thereof.
  • one or more doses of an agent in a kit described herein are provided in the form of a vial, bottle, or capsule.
  • a system for measuring water concentration in a sample includes a membrane that is transparent to one or more forms of radiation in at least one region of interest, an enclosure that removably retains the membrane and includes an optically transmissive region through which radiation may pass, and an inlet for the enclosure.
  • a system described herein further includes a pump.
  • a pump is capable of one or more of creating a vacuum, and introducing a gas that is substantially free of water into and/or through at least a portion of the enclosure.
  • a system described herein further includes a cooling means.
  • a cooling means is or includes a metal holder surrounded by a reservoir containing a cooling fluid and/or a cooling means is or includes an external chiller that cools a fluid, which is circulated through a jacket surrounding a membrane assembly.
  • a system further includes a porous support for a membrane.
  • an inlet of a system described herein includes a connector.
  • a system described herein further includes one or more seals.
  • Figure 1 depicts an exemplary picture and schematic of a stainless-steel membrane assembly in accordance with one or more embodiments of the present disclosure
  • Figure 2 depicts an exemplary picture and schematic of a sample holder in accordance with one or more embodiments of the present disclosure
  • Figure 3 depicts exemplary plots of infrared spectra of water in CCl 4 (Panel A), power steering fluid (Panel B), vegetable oil (Panel C), and EP fluid (Panel D) in accordance with one or more embodiments of the present disclosure
  • Figure 4 is an exemplary plot of infrared spectra of (a) water in a vegetable oil sample (3 mL, 10 ppm), (b) water in a power steering oil sample (3 mL, 10 ppm), (b) water in a power steering oil sample (3 mL, 10 ppm), (b) water in a power steering oil sample (3 mL, 10 ppm), (b) water in a power steering oil sample (3 mL
  • the term “approximately” or “about” refers to a range of values that fall within 25 %, 20 %, 19 %, 18 %, 17 %, 16 %, 15 %, 14 %, 13 %, 12 %, 11 %, 10 %, 9 %, 8 %, 7 %, 6 %, 5 %, 4 %, 3 %, 2 %, 1 %, or less in either direction (greater than or less than) of the stated reference value unless otherwise stated or otherwise evident from the context (except where such number would exceed 100 % of a possible value). [0072] Determine: Many methodologies described herein include a step of “determining”.
  • determining can utilize or be accomplished through use of any of a variety of techniques available to those skilled in the art, including for example specific techniques explicitly referred to herein.
  • determining involves manipulation of a physical sample.
  • determining involves consideration and/or manipulation of data or information, for example utilizing a computer or other processing unit adapted to perform a relevant analysis.
  • determining involves receiving relevant information and/or materials from a source.
  • determining involves comparing one or more features of a sample or entity to a comparable reference
  • substantially refers to the qualitative condition of exhibiting total or near-total extent or degree of a characteristic or property of interest.
  • biological and chemical phenomena rarely, if ever, go to completion and/or proceed to completeness or achieve or avoid an absolute result.
  • the term “substantially” is therefore used herein to capture the potential lack of completeness inherent in many biological and chemical phenomena.
  • compositions, compounds, or products are described as having, including, or comprising specific components, or where processes and methods are described as having, including, or comprising specific steps, it is contemplated that, additionally, there are articles, devices, and systems of the present application that consist essentially of, or consist of, recited components, and that there are processes and methods according to the present application that consist essentially of, or consist of, recited processing steps.
  • order of steps or order for performing certain actions is immaterial so long as a described method remains operable. Moreover, two or more steps or actions may be conducted simultaneously.
  • water existing in a sample as dissolved water or emulsified water droplets is extracted using a membrane that is transparent to one or more form(s) of radiation in at least one region of interest.
  • water may form an adsorbed layer on the membrane and produces a typical spectrum of water.
  • no calibration or additional reagents are required for this approach.
  • this approach may be used over a detection range of 1 to 5000 ppm of water.
  • one or more reagents that react with and/or adsorb water is added to a sample.
  • a reaction and/or adsorption product is collected and quantified to determine water concentration of the sample.
  • a region of interest includes a range of wavelengths at which water and/or a reaction and/or adsorption product of water absorb radiation.
  • a sample is processed through a membrane that is transparent to one or more forms of radiation in at least one region of interest, the membrane is irradiated with the one or more forms of radiation, and the water concentration in the sample is determined from one or more absorbance and/or Raman peaks.
  • A. Samples i. Composition of sample [0083]
  • a sample is a hydrophobic sample.
  • a sample is or comprises an oil or a solvent.
  • a sample is or comprises an oil.
  • an oil is selected from the group consisting of a lubricating oil, vegetable oil, animal-based oil, hydraulic oil, petroleum-based oil, heavy gas (e.g.
  • an oil is or comprises a power steering fluid.
  • an oil is or comprises a vegetable oil (e.g. Olive and Soya bean oil).
  • an oil is or comprises an animal-based oil (e.g., fish oil).
  • an oil is or comprises an extreme pressure oil (e.g. gear oil).
  • an oil is or comprises a petroleum- based oil.
  • an oil is or comprises a mixture of a petroleum-based oil and a synthetic oil (e.g., an aviation fuel).
  • a petroleum-based oil is or comprises an oil selected from the group consisting of crude oil, gasoline, kerosene, diesel oil, aviation fuel, racing fuel, and vacuum residue fuel (VR fuel, e.g., the heaviest fraction of oil produced during the distillation of crude oils).
  • an oil is or comprises crude oil.
  • an oil is or comprises gasoline.
  • an oil is or comprises kerosene.
  • an oil is or comprises diesel oil.
  • an oil is or comprises racing fuel (e.g. VP racing fuel).
  • an oil is or comprises VR fuel.
  • an oil is or comprises heavy gas.
  • heavy gas is or comprises sulfur hexafluoride.
  • an oil is or comprises synthetic oil.
  • an oil is or comprises an oil additive.
  • an oil is or comprises biofuel.
  • an oil is or comprises waste oil (e.g. RCRA waste oil).
  • a sample is or comprises a solvent.
  • a solvent is or comprises a non-aqueous solvent.
  • a solvent is or comprises an organic solvent.
  • an organic solvent is selected from the group consisting of an alcohol, a hydrocarbon, a halogenated solvent, a ketone, an ether, a glycol, a nitrogen- containing solvent, a sulfur-containing solvent, a furyl solvent, an aromatic solvent, a silane liquid, an ionic liquid, and combinations thereof.
  • an alcohol is selected from the group consisting of methanol, ethanol, propanol, isopropanol, butanol, and the like.
  • a hydrocarbon is selected from the group consisting of pentane, hexane, heptane, octane, and the like.
  • a halogenated solvent is a chlorinated solvent.
  • a chlorinated solvent is selected from the group consisting of chloroform, dichloromethane, dichloroethane, and the like.
  • a ketone is selected from the group consisting of acetone, methyl ethyl ketone, methyl isobutyl ketone, diisobutyl ketone, cyclohexanone, and the like.
  • an ether is selected from the group consisting of diethyl ether, methyl tert-butyl ether, tetrahydrofuran, dioxane, and the like.
  • a glycol is selected from the group consisting of ethylene glycol, propylene glycol, and the like.
  • a nitrogen-containing solvent is selected from the group consisting of pyridine, triethylamine, imidazole, acetonitrile, urea, and the like.
  • a sulfur-containing solvent is selected from the group consisting of dimethyl sulfoxide and the like.
  • a furyl solvent is selected from furfural and the like.
  • an aromatic solvent is selected from the group consisting of benzene, toluene, xylene, and the like.
  • a silane liquid is selected from the group consisting of alkyltrimethoysilane, alkyltrichlorosilane, and polydimethylsilicone oil.
  • an ionic liquid is selected from the group consisting of 1-ethyl-3- methylimidazolium, ethylammonium nitrate and 1-alkylpyridinium.
  • Concentration range of water in sample [0085] In some embodiments, water concentration in a sample is in the range of about 1 ppm to about 10,000 ppm. In some embodiments, water concentration in a sample is in the range of about 1 ppm to about 5,000 ppm.
  • water concentration in a sample is in the range of about 1 ppm to about 1,000 ppm. In some embodiments, water concentration in a sample is in the range of about 1 ppm to about 500 ppm. In some embodiments, water concentration in a sample is in the range of about 1 ppm to about 100 ppm. In some embodiments, water concentration in a sample is in the range of about 1 ppm to about 10 ppm. In some embodiments, water concentration in a sample is in the range of about 10 ppm to about 5,000 ppm. In some embodiments, water concentration in a sample is in the range of about 10 ppm to about 1,000 ppm.
  • water concentration in a sample is in the range of about 10 ppm to about 500 ppm. In some embodiments, water concentration in a sample is in the range of about 10 ppm to about 100 ppm. In some embodiments, water concentration in a sample is in the range of about 100 ppm to about 5,000 ppm. In some embodiments, water concentration in a sample is in the range of about 100 ppm to about 1,000 ppm. In some embodiments, water concentration in a sample is in the range of about 1,000 ppm to about 10,000 ppm. In some embodiments, water concentration in a sample is in the range of about 1,000 ppm to about 5,000 ppm.
  • a membrane is transparent to one or more forms of radiation in at least one region of interest. In some embodiments, a membrane is transparent to one or more forms of radiation in at least one region of interest, wherein the one or more forms of radiation comprises microwave, infrared, visible, and/or ultraviolet light. In some embodiments, a membrane is transparent to microwave light in at least one region of interest. In some embodiments, a membrane is transparent to infrared light in at least one region of interest. In some embodiments, a membrane is transparent to visible light in at least one region of interest.
  • a membrane is transparent to ultraviolet light in at least one region of interest.
  • a membrane has a diameter in the range of about 1 to about 100 mm. In some embodiments, a membrane has a diameter in the range of about 1 to about 80 mm. In some embodiments, a membrane has a diameter in the range of about 1 to about 50 mm. In some embodiments, a membrane has a diameter in the range of about 1 to about 30 mm. In some embodiments, a membrane has a diameter in the range of about 5 to about 30 mm. In some embodiments, a membrane has a diameter in the range of about 10 to about 50 mm.
  • a membrane has a diameter in the range of about 10 to about 41 mm. In some embodiments, a membrane has a diameter in the range of about 10 to about 30 mm. In some embodiments, a membrane has a diameter of about 10 mm, about 11 mm, about 12 mm, about 13 mm, about 14 mm, about 15 mm, about 16 mm, about 17 mm, about 18 mm, about 19 mm, about 20 mm, about 21 mm, about 22 mm, about 23 mm, about 24 mm, about 25 mm, about 26 mm, about 27 mm, about 28 mm, about 29 mm, or about 30 mm. [0088] In some embodiments, a membrane is characterized in terms of its void volume.
  • a volume of sample applied to a membrane is at least 10 times the void volume of said membrane.
  • a membrane has a void volume of about 1 to about 50 ⁇ L.
  • a membrane has a void volume of about 1 to about 40 ⁇ L.
  • a membrane has a void volume of about 10 to about 40 ⁇ L.
  • a membrane has a void volume of about 15 to about 35 ⁇ L. It will be appreciated by a person of skill in the art that void volume of a membrane is related to membrane diameter and thickness; for example, void volume is proportional to the square of the membrane diameter. [0089]
  • a membrane is or comprises a metal mesh membrane.
  • a membrane is or comprises a steel mesh membrane. In some embodiments, a membrane is or comprises a glass fiber membrane. In some embodiments, a membrane is or comprises a polymer membrane. In some embodiments, a membrane is or comprises a polyethylene or a polypropylene membrane. In some embodiments, a membrane is or comprises a polytetrafluoroethylene membrane (eg a Teflon TM membrane) In some embodiments a membrane is or comprises a hydrophobic polytetrafluoroethylene membrane (e.g. a hydrophobic Teflon TM membrane). In some embodiments, a membrane is or comprises a hydrophilic polytetrafluoroethylene membrane (e.g.
  • a membrane is or comprises a metal-coated polymer membrane.
  • a membrane is coated in an agent that reacts and/or adsorbs water.
  • selection of a membrane material that has a refractive index near the refractive index of a sample and/or water provides for a membrane that is particularly well suited for use in methods encompassed by the present disclosure. Without wishing to be held to a particular theory, it is contemplated that use of such membranes may be helpful in providing a membrane that is transparent to one or more form of radiation in at least one area of interest.
  • any of a variety of application- appropriate materials may be used in or as membranes in provided methods and systems.
  • some such materials are disclosed in U.S. Patent No. 10,031,136, the entirety of which is hereby incorporated by reference.
  • a membrane may be incorporated into a membrane assembly.
  • a membrane may be removably inserted into a membrane assembly.
  • a membrane assembly comprises a membrane, a support for the membrane (e.g., a porous support), and, optionally, an enclosure with one or more inlet(s) and/or outlet(s).
  • a support for a membrane is or comprises any form of support for the membrane that provides mechanical stability to a membrane.
  • a support for a membrane prevents the membrane from tearing or falling from its position.
  • a support for a membrane provides for a membrane to be maintained in a desired position.
  • a membrane assembly further comprises one or more sealing component(s).
  • a sealing component provides a seal to a membrane assembly to prevent leakage of one or more substances (e.g. a gas or a liquid) into and/or out of a membrane assembly.
  • a sealing component is or comprises an O-ring seal.
  • a sealing component is or comprises aluminum, copper, bronze, or combinations thereof.
  • a sealing component is or comprises glue paste (e.g. Flex Paste TM ).
  • a sealing component is or comprises tape (e.g. Flex Tape TM , Teflon TM tape).
  • the inlet of the membrane assembly is or comprises a connector (e.g. a Luer TM lock, a slip tip connector).
  • a connector allows for functional connection between components of a membrane assembly and/or functional connection of a membrane assembly to an external component.
  • a membrane assembly is or comprises metal.
  • a membrane assembly comprises a metal enclosure and/or metal porous support for the membrane.
  • a membrane assembly is or comprises plastic.
  • a membrane assembly comprises a plastic enclosure and/or plastic support for the membrane.
  • a membrane assembly is designed for single-use and/or is disposable.
  • An example membrane assembly is depicted in Figure 1.
  • C. Radiation Many of the methods described herein use one or more form(s) of radiation to produce one or more absorbance and/or Raman peaks for the quantification of water in a sample.
  • a form of radiation useful in, for example, provided methods is or comprises microwave, infrared, visible, or ultraviolet light.
  • a form of radiation useful in, for example, provided methods is or comprises microwave light.
  • a form of radiation has a wavelength in the range of about 1 mm to about 100 cm. In some embodiments, a form of radiation is or comprises extremely high frequency microwaves. In some embodiments, a form of radiation has a wavelength in the range of about 1 mm to about 10 mm. In some embodiments, a form of radiation is or comprises super high frequency microwaves. In some embodiments, a form of radiation has a wavelength in the range of about 10 mm to about 20 cm. In some embodiments, a form of radiation has a wavelength in the range of about 1 cm to about 15 cm. In some embodiments, a form of radiation has a wavelength in the range of about 10 mm to about 10 cm.
  • a form of radiation is or comprises ultra-high frequency microwaves. In some embodiments, a form of radiation has a wavelength in the range of about 10 cm to about 100 cm. In some embodiments a form of radiation has a wavelength of about 10 cm to about 20 cm. In some embodiments, a form of radiation has a wavelength of about 12.24 cm. In some embodiments, a form of radiation has a wavelength of about 5.16 cm. In some embodiments, a form of radiation has a wavelength of about 1.24 cm. ii. Infrared (IR) Light [0094] In some embodiments, a form of radiation useful in, for example, provided methods, is or comprises infrared light.
  • a form of radiation has a wavelength in the range of about 700 nm to about 1 mm. In some embodiments, a form of radiation is or comprises far-infrared light. In some embodiments, a form of radiation has a wavelength in the range of about 25 ⁇ m to about 1 mm. In some embodiments, a form of radiation is or comprises mid-infrared light. In some embodiments, a form of radiation has a wavelength in the range of about 2.5 ⁇ m to about 25 ⁇ m. In some embodiments, a form of radiation is or comprises near- infrared light. In some embodiments, a form of radiation has a wavelength in the range of about 700 nm to about 2.5 ⁇ m. iii.
  • a form of radiation useful in, for example, provided methods is or comprises visible light. In some embodiments, a form of radiation has a wavelength in the range of about 380 to about 700 nm. iv. Ultraviolet (UV) Light [0096] In some embodiments, a form of radiation useful in, for example, provided methods, is or comprises ultraviolet light. In some embodiments, a form of radiation has a wavelength in the range of about 10 nm to about 380 nm. In some embodiments, a form of radiation is or comprises near-ultraviolet light. In some embodiments, a form of radiation has a wavelength in the range of about 300 nm to about 380 nm.
  • a form of radiation is or comprises mid-ultraviolet light. In some embodiments, a form of radiation has a wavelength in the range of about 200 nm to about 300 nm. In some embodiments, a form of radiation is or comprises far ultraviolet light. In some embodiments, a form of radiation has a wavelength in the range of about 100 nm to about 200 nm. In some embodiments, a form of radiation is or comprises extreme ultraviolet light. In some embodiments, a form of radiation has a wavelength in the range of about 10 nm to about 100 nm. D.
  • one or more absorbance and/or Raman peak(s) are used to measure water concentration in a sample.
  • an absorbance peak is measured from reflected, transmitted, emitted, scattered light, or combinations thereof.
  • an absorbance peak is measured from reflected light.
  • an absorbance peak is measured from transmitted light.
  • an absorbance peak is measured from emitted light.
  • an absorbance peak is measured from scattered light.
  • one or more absorbance and/or Raman peaks are measured using a device (e.g. spectrometer).
  • one or more absorbance and/or Raman peaks are measured with a Fourier Transform Infrared Spectrometer (FTIR), a single-beam dispersive infrared spectrometer, a double-beam dispersive infrared spectrometer, a filtermetric spectrometer, a tunable laser based infrared spectrometer, or a Raman spectrometer.
  • FTIR Fourier Transform Infrared Spectrometer
  • FTIR Fourier Transform Infrared Spectrometer
  • one or more absorbance peaks are measured with a single-beam dispersive infrared spectrometer.
  • one or more absorbance peaks are measured with a double-beam dispersive infrared spectrometer. In some embodiments, one or more absorbance peaks are measured with a filtermetric spectrometer. In some embodiments, one or more absorbance peaks are measured with a tunable laser based infrared spectrometer. In some embodiments, one or more Raman peaks are measured with a Raman spectrometer. In some embodiments, one or more absorbance peaks are measured with a UV/Vis spectrometer. In some embodiments, a UV/Vis spectrometer is a dispersive, MEMS-based, filtermetric, and/or tunable laser-based spectrometer.
  • one or more absorbance peaks are measured with a microwave spectrometer. In some embodiments, one or more absorbance peaks are measured using a radiometric-based system. In some embodiments, a radiometric-based system produces a single wavelength, for example, 12.24 cm.
  • the present disclosure is directed to methods of measuring water concentration in a sample comprising steps of passing a sample through a membrane that is transparent to one or more forms of radiation in at least one region of interest, irradiating the membrane with the one or more forms of radiation, and determining water concentration in the sample from one or more absorbance and/or Raman peaks. i.
  • Water Retention Management (e.g., cooling)
  • a step of passing a sample through a membrane results in extraction of water from the sample and adsorption of a water layer to the membrane.
  • the membrane is cooled (e.g., to a temperature of 10 o C or lower) prior to the step of passing the sample through the membrane and/or for at least a portion of the passing, irradiating, and determining steps in order to prevent evaporation of the water layer adsorbed to the membrane.
  • cooling a membrane or membrane assembly to prevent evaporation of the adsorbed water layer increases accuracy and precision of quantification of water content of an oil sample.
  • a membrane or membrane assembly is cooled to a temperature between about -196°C to about 10 °C, inclusive.
  • a membrane or membrane assembly is cooled to a temperature between about -79°C to about 10 °C, inclusive. In some embodiments, a membrane or membrane assembly is cooled to a temperature between about -79°C to about 0 °C, inclusive. In some embodiments, a membrane or membrane assembly is cooled to a temperature between about -20°C to about 0 °C, inclusive. In some embodiments, a membrane or membrane assembly is cooled to a temperature of about -196 °C. In some embodiments, a membrane or membrane assembly is cooled to a temperature of about -78 °C. In some embodiments, a membrane or membrane assembly is cooled to a temperature of about -20 °C.
  • a membrane or membrane assembly is cooled to a temperature of about -15 °C. In some embodiments, a membrane or membrane assembly is cooled to a temperature of about -10 °C. In some embodiments, a membrane or membrane assembly is cooled to a temperature of about -5 °C. In some embodiments, a membrane or membrane assembly is cooled to a temperature of about 0 °C. In some embodiments, a membrane or membrane assembly is cooled with dry ice. In some embodiments, a membrane or membrane assembly is cooled with dry ice and acetone. In some embodiments, a membrane or membrane assembly is cooled with dry ice and isopropanol. In some embodiments, a membrane or membrane assembly is cooled with ice.
  • a membrane or membrane assembly is cooled with ice and sodium chloride. In some embodiments, a membrane or membrane assembly is cooled with liquid nitrogen. [0103] It will be appreciated that retention of water on a membrane, as extracted from a sample, for a length of time necessary to perform the methods described herein is an important step so as to prevent artificial skewing of results. Without wishing to be bound by any particular theory, it is believed that pre-cooling a membrane or membrane assembly (e.g. cooling a membrane prior to the step of passing the sample through the membrane) may prevent evaporation of adsorbed water from the membrane for the entire length of time required for performing a method described herein. For example, a method described herein may take up to 5 minutes to complete.
  • pre-cooling a membrane or membrane assembly prevents evaporation of adsorbed water from the membrane for at least about 5 minutes. In some embodiments, pre-cooling a membrane or membrane assembly prevents evaporation of adsorbed water from the membrane for at least about 6 minutes.
  • Exogenous Water Management e.g., vacuum and/or gas exposure
  • Two exemplary ways of managing exogenous water formation during or after cooling are through application of vacuum to a membrane or membrane assembly and/or exposure of a membrane to an inert or dry gas.
  • a membrane or membrane assembly is purged with a gas that is substantially free of water prior to the step of passing the sample through the membrane. Without wishing to be held to a particular theory, it is contemplated that circulation of such a gas prior to passing of the sample through the membrane prevents exposure to and/or condensation of atmospheric water on the membrane.
  • a gas that is substantially free of water is selected from the group consisting of dry air, a dry inert gas, hydrogen gas, or dry carbon dioxide.
  • a gas that is substantially free of water is or comprises dry air.
  • a gas that is substantially free of water is or comprises hydrogen gas. In some embodiments, a gas that is substantially free of water is or comprises dry carbon dioxide. In some embodiments, an inert gas is selected from N 2 , Argon, Helium, Neon, Krypton, or Xenon. In some embodiments, a gas that is substantially free of water is afforded by attaching a compressed gas to a commercial dryer. For example, in some embodiments, compressed air is attached to a Balston Compressed Air Dryer for use in one or more methods described herein. [0105] In some embodiments, a membrane or membrane assembly is subjected to vacuum while cooling and/or prior to the step of passing a sample through the membrane.
  • a membrane or membrane assembly is inserted into a cooling stage and evacuated prior to the step of passing the sample through the membrane.
  • a cooling stage is or comprises a metal holder surrounded by a reservoir that is in functional contact with the metal holder.
  • a reservoir includes a cooling fluid (e.g. antifreeze, dry ice, liquid nitrogen, and the like).
  • a cooling stage fits in a sample compartment of a spectrometer, for example, without impeding the path of a light beam through a membrane assembly.
  • a cooling fluid is circulated through a housing that is in contact with a membrane assembly.
  • a cooling fluid is cooled using an external chiller, circulated through a jacket functionally connected to a membrane assembly, then returned to the external chiller to be cooled again and recirculated.
  • a membrane or membrane assembly is cooled in an enclosure with a controlled atmosphere, such as a controlled-atmosphere glovebox, prior to the step of passing the sample through a membrane.
  • a controlled- atmosphere glovebox is an inert atmosphere glovebox.
  • a controlled- atmosphere glovebox is a low humidity glovebox.
  • iii. Management of Water Retention and Exogenous Water Formation During Data Collection [0107] Without being bound by any particular theory, it is believed that cooling a membrane or membrane assembly during the steps of the methods described herein can prolong the length of water retention on a membrane and enable data collection over longer periods of time without skewing of results.
  • a membrane or membrane assembly is cooled for at least a portion of the passing, irradiating, and/or determining steps.
  • a membrane or membrane assembly is cooled for at least a portion of the passing step.
  • a membrane or membrane assembly is cooled for at least a portion of the irradiating step.
  • a membrane or membrane assembly is cooled for at least a portion of the determining step. In some embodiments, a membrane or membrane assembly is continuously cooled through the passing, irradiating, and determining steps. In some embodiments, a membrane or membrane assembly is continuously cooled by pumping a chilled fluid through a jacket surrounding the enclosure of the membrane assembly. Examples of commercially available chillers include Mokon Full Range Heating and Chilling Systems, TC Series Central Chillers, Chiller Systems from Dry Coolers, Inc., and 5HP Industrial Water Cooled Chiller 460V 3-P. Without wishing to be bound by any particular theory, it is believed that continuously cooling a membrane or membrane assembly during data collection will substantially prevent evaporation of water from the membrane.
  • continuous cooling of a membrane or membrane assembly can enable use of plastic membrane assemblies.
  • plastic which is not thermally conductive, in a membrane assembly, likely results in evaporation of adsorbed water within one minute. Accordingly, without use of some cooling or other means, plastic membrane assemblies may not be compatible with various embodiments.
  • Absorbance and/or Raman Peaks [0108] Depending upon the methods used, observing absorbance and/or Raman peaks of a particular wavelength is considered indicative of the presence of some amount of water in a sample.
  • the presence of water in a sample may be indicated by one or more absorbance and/or Raman peaks are characterized in that they occur at a wavelength selected from the group consisting of about 5185 cm -1 , about 3420 cm -1 , about 2127 cm -1 , about 1650 cm -1 , about 800 cm -1 and combinations thereof.
  • the presence of water in a sample is indicated by one or more absorbance and/or Raman peaks are characterized in that they occur at a wavelength of about 5185 cm -1 .
  • the presence of water in a sample is indicated by one or more absorbance and/or Raman peaks are characterized in that they occur at a wavelength of about 3420 cm -1 .
  • the presence of water in a sample is indicated by one or more absorbance and/or Raman peaks are characterized in that they occur at a wavelength of about 2127 cm -1 .
  • the presence of water in a sample is indicated by one or more absorbance and/or Raman peaks are characterized in that they occur at a wavelength of about 1650 cm -1 .
  • the presence of water in a sample is indicated by one or more absorbance and/or Raman peaks are characterized in that they occur at a wavelength of about 800 cm -1 .
  • the one or more absorbance and/or Raman peaks are characterized by a wavelength of about 3420 cm -1 .
  • the one or more absorbance and/or Raman peaks are characterized by a wavelength of about 2127 cm -1 .
  • the presence of water in a sample may be indicated by one or more absorbance and/or Raman peaks are characterized in that they occur at a wavelength selected from the group consisting of about 10 nm to about 380 nm.
  • the presence of water in a sample may be indicated by one or more absorbance and/or Raman peaks are characterized in that they occur at a wavelength selected from the group consisting of about 190 to 320 nm.
  • the presence of water in a sample may be indicated by one or more absorbance peaks are characterized in that they occur at a wavelength selected from the group consisting of about 1 mm to about 100 cm, and combinations thereof.
  • the presence of water in a sample is indicated by one or more absorbance peaks are characterized in that they occur at a wavelength of about 1.24, about 5.16, about 12.24 cm, and combinations thereof.
  • the present disclosure is directed to methods of measuring water concentration in a sample comprising steps of adding an agent to a sample to react with and/or adsorb water from the sample, thereby forming a solid particulate material; collecting the solid particulate material on a membrane that is transparent to one or more forms of radiation in at least one region of interest; irradiating the membrane with the one or more forms of radiation; and determining water concentration in the sample from one or more absorbance and/or Raman peaks.
  • the present disclosure is directed to methods of measuring water concentration in a sample comprising steps of adding an agent to a sample to react with water from the sample, thereby forming a solid particulate material; collecting the solid particulate material on a membrane that is transparent to one or more forms of radiation in at least one region of interest; irradiating the membrane with the one or more forms of radiation; and determining water concentration in the sample from one or more absorbance and/or Raman peaks.
  • the present disclosure is directed to methods of measuring water concentration in a sample comprising steps of adding an agent to a sample to adsorb water from the sample, thereby forming a solid particulate material; collecting the solid particulate material on a membrane that is transparent to one or more forms of radiation in at least one region of interest; irradiating the membrane with the one or more forms of radiation; and determining water concentration in the sample from one or more absorbance and/or Raman peaks.
  • the present disclosure is directed to methods of measuring water concentration in a sample comprising steps of adding a membrane that is transparent to one or more forms of radiation in at least one region of interest and coated in an agent to a sample to react with and/or adsorb water from the sample thereby extracting water from the sample; irradiating the membrane with the one or more forms of radiation; and determining water concentration in the sample from one or more absorbance and/or Raman peaks.
  • the present disclosure is directed to methods of measuring water concentration in a sample comprising steps of adding an agent to a sample to react with and/or adsorb water from the sample, thereby forming a solid particulate material; collecting the solid particulate material by centrifugation; depositing the solid particulate material on a membrane that is transparent to one or more forms of radiation in at least one region of interest; irradiating the membrane with the one or more forms of radiation; and determining water concentration in the sample from one or more absorbance and/or Raman peaks.
  • the present disclosure is directed to methods of measuring water concentration in a sample comprising steps of adding an agent to a sample to react with and/or adsorb water from the sample, thereby forming a solid particulate material; collecting the solid particulate material by centrifugation; sampling the solid particulate materials by one or more spectroscopic techniques; and determining water concentration in the sample from one or more absorbance and/or Raman peaks.
  • a spectroscopic technique is selected from the group consisting of transmission, attenuated total reflectance (ATR), diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), specular reflectance or photoacoustic infrared spectroscopy, Raman spectroscopy, UV-vis spectroscopy, and microwave spectroscopy.
  • ATR attenuated total reflectance
  • DRIFTS diffuse reflectance infrared Fourier transform spectroscopy
  • specular reflectance or photoacoustic infrared spectroscopy Raman spectroscopy
  • UV-vis spectroscopy UV-vis spectroscopy
  • microwave spectroscopy microwave spectroscopy
  • the present disclosure is directed to methods of measuring water concentration in a sample comprising steps of adding an agent contained in a porous enclosure to a sample to react with and/or adsorb water from the sample, for example, to form a solid particulate material contained in the porous enclosure; removing the porous enclosure; sampling the solid particulate material by one or more spectroscopic techniques; and determining water concentration in the sample from one or more absorbance and/or Raman peaks.
  • a spectroscopic technique is selected from the group consisting of transmission, attenuated total reflectance (ATR), diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), specular reflectance or photoacoustic infrared spectroscopy, Raman spectroscopy, UV- vis spectroscopy, and microwave spectroscopy.
  • the present disclosure is directed to methods of measuring water concentration in a sample comprising steps of adding a magnetic particulate material coated in an agent to a sample to react with and/or adsorb water from the sample, thereby extracting water from the sample; collecting the magnetic particulate material with a magnet; depositing the magnetic particulate material on a membrane that is transparent to one or more forms of radiation in at least one region of interest; irradiating the membrane with the one or more forms of radiation; and determining water concentration in the sample from one or more absorbance and/or Raman peaks.
  • an agent added to a sample is in the form of a powder.
  • an agent added to a sample is in the form of a coating on a membrane.
  • an agent is selected from the group consisting of, but not limited to calcium oxide, magnesium oxide, copper sulfate, zinc oxide, sodium oxide, iron chloride, cobalt nitrate, nickel sulfate, tungsten oxide, alumina, silica, titania, calcium hydride, and combinations thereof.
  • an agent is or comprises calcium oxide.
  • an agent is or comprises magnesium oxide.
  • an agent is or comprises copper sulfate.
  • an agent may be a hydrate of copper sulfate; for example, a mono-, di-, tri- or tetrahydrate of copper sulfate may be added.
  • an agent is or comprises zinc oxide.
  • an agent is or comprises sodium oxide.
  • an agent is or comprises iron chloride.
  • an agent is or comprises cobalt nitrate.
  • an agent is or comprises nickel sulfate.
  • an agent is or comprises tungsten oxide.
  • an agent is or comprises alumina.
  • an agent is or comprises titania.
  • an agent is or comprises calcium hydride.
  • an amount of agent is added such that absence of an absorbance peak at 3420 cm -1 indicates complete consumption of water in the sample.
  • formation of a reaction and/or absorption product of an agent with water is indicated by one or more absorbance and/or Raman peaks are characterized by a wavelength in the range of about 50 to about 6000 cm -1 .
  • Ca(OH) 2 reacts with water to form Ca(OH) 2 .
  • formation of Ca(OH) 2 is indicated by one or more absorbance and/or Raman peaks characterized by a wavelength of about 450, 875, 1443 and 3645 cm -1 , or combinations thereof.
  • formation of Ca(OH) 2 is indicated by one or more Raman peaks characterized by a wavelength of about 796 cm -1 , about 913 cm -1 , about 1187 cm -1 , and combinations thereof.
  • formation of Ca(OH) 2 is indicated by one or more absorbance and/or Raman peaks characterized by a wavelength of about 450 nm.
  • Copper sulfate [0120]
  • copper sulfate adsorbs water to form a hydrate as an adsorption product.
  • a hydrate of copper sulfate formed as an adsorption product with water is selected from copper sulfate monohydrate, copper sulfate dihydrate, copper sulfate trihydrate, copper sulfate tetrahydrate, copper sulfate pentahydrate, and combinations thereof.
  • a hydrate of copper sulfate formed as an adsorption product with water is copper sulfate monohydrate. In some embodiments, a hydrate of copper sulfate formed as an adsorption product with water is copper sulfate pentahydrate. [0121] In some embodiments, formation of a copper sulfur hydrate is indicated by one or more absorbance and/or Raman peaks are characterized by a wavelength in a range of about 3500 cm -1 to about 3100 cm -1 , in a range of about 1600 cm -1 to about 1800 cm -1 , or combinations thereof.
  • formation of a copper sulfur hydrate is indicated by one or more absorbance and/or Raman peaks are characterized by a wavelength of about 3420 cm -1 , 3190 cm -1 , 1743 cm -1 , 1667 cm -1 , or combinations thereof.
  • formation of a copper sulfur hydrate is indicated by one or more absorbance and/or Raman peaks are characterized by a wavelength of about 3420 cm -1 .
  • formation of a copper sulfur hydrate is indicated by one or more absorbance and/or Raman peaks are characterized by a wavelength of about 3190 cm -1 .
  • formation of a copper sulfur hydrate is indicated by one or more absorbance and/or Raman peaks are characterized by a wavelength of about 1743 cm -1 . In some embodiments, formation of a copper sulfur hydrate is indicated by one or more absorbance and/or Raman peaks are characterized by a wavelength of about 1667 cm -1 .
  • formation of a copper sulfur hydrate is indicated by one or more Raman peaks characterized by a wavelength of about 125 cm -1 , about 280 cm -1 , about 455 cm -1 , about 611 cm -1 , about 984 cm -1 , about 1146 cm- 1 , about 3110 cm -1 , about 3190 cm -1 , about 3355 cm -1 , about 3475 cm -1 , or combinations thereof.
  • formation of a copper sulfur hydrate is indicated by one or more absorbance and/or Raman peaks characterized by a wavelength of about 800 nm.
  • an agent added to a sample is copper sulfate, and wherein copper sulfate adsorbs water to form a copper sulfate monohydrate
  • one or more absorbance and/or Raman peaks are characterized by a wavelength of about 3190 cm -1 , about 1743 cm -1 , or combinations thereof.
  • one or more absorbance and/or Raman peaks are characterized by a wavelength of about 3190 cm- 1.
  • an agent added to a sample is copper sulfate, and wherein copper sulfate adsorbs water to form a copper sulfate monohydrate, one or more absorbance and/or Raman peaks are characterized by a wavelength of about 1743 cm -1 .
  • the present disclosure is directed to kits for measuring water concentration in a sample.
  • a kit as provided herein may comprise any of the components described elsewhere in this disclosure.
  • a kit for measuring water concentration comprises: one or more doses of an agent and a membrane assembly containing a membrane (e.g., a membrane is transparent to one or more forms of radiation in at least one region of interest).
  • a dose of an agent is provided in a vial, capsule, bottle, and the like.
  • a capsule dissolves upon contact with an oil sample to exposure the agent to the oil sample.
  • a system for measuring water concentration in a sample comprises a membrane that is transparent to one or more forms of radiation in at least one region of interest, an enclosure that retains and/or removably retains the membrane and includes an optically transmissive region through which radiation may pass, and one or more inlet(s) and/or outlet(s) for the enclosure.
  • a system for measuring water concentration in a sample comprises a membrane that is transparent to one or more forms of radiation in at least one region of interest, an enclosure that retains the membrane and includes an optically transmissive region through which radiation may pass, and one or more inlet(s) and/or outlet(s) for the enclosure.
  • a system for measuring water concentration in a sample comprises a membrane that is transparent to one or more forms of radiation in at least one region of interest, an enclosure that removably retains the membrane and includes an optically transmissive region through which radiation may pass, and one or more inlet(s) and/or outlet(s) for the enclosure.
  • An optically transmissive region may be comprised of any application-appropriate material.
  • an open space or comprise glass, plastic, salts, silicon, germanium, or the like, so long as it allows one or more particular wavelength(s) of radiation to pass through.
  • a salt may comprise NaCl, ZnSe, CaF 2 , or the like.
  • an enclosure is or comprises a housing. In some embodiments, an enclosure is or comprises a metal housing. In some embodiments, an enclosure is or comprises a plastic housing. [0126] In some embodiments, an inlet and/or outlet in an enclosure is or comprises a connector. In some embodiments, a connector allows for functional connection between components of a membrane assembly and/or functional connection of a membrane assembly to an external component. In some embodiments, a connector is a Luer TM lock. In some embodiments, a connector is a slip tip connector. [0127] In some embodiments, a system further comprises a pump. In some embodiments, an inlet and/or outlet of an enclosure is adapted for attachment to a pump.
  • a pump is capable of one or more of: creating a vacuum, and introducing a gas that is substantially free of water into and/or through at least a portion of the enclosure
  • a system further comprises a cooling means.
  • a cooling means is or comprises a jacket surrounding the enclosure of the membrane assembly through which a chilled fluid is pumped. Examples of commercially available chillers include Mokon Full Range Heating and Chilling Systems, TC Series Central Chillers, Chiller Systems from Dry Coolers, Inc., and 5HP Industrial Water Cooled Chiller 460V 3-P.
  • a system further comprises a support for the membrane (e.g. a porous support).
  • a support for a membrane is or comprises any form of support for the membrane that provides mechanical stability to a membrane.
  • a support for a membrane prevents the membrane from tearing or falling from its position.
  • a support for a membrane provides for a membrane to be maintained in a desired position.
  • the porous support is or comprises metal.
  • the porous support is or comprises plastic.
  • a membrane support is transparent in one or more regions of interest.
  • a system further comprises one or more sealing component(s).
  • a sealing component provides a seal to a membrane assembly to prevent leakage of one or more substances (e.g.
  • a sealing component is or comprises an O-ring seal.
  • a sealing component is or comprises aluminum, copper, bronze, or combinations thereof.
  • a sealing component is or comprises glue paste (e.g. Flex Paste TM ).
  • a sealing component is or comprises tape (e.g. Flex Tape TM , Teflon TM tape).
  • quantification can be performed by any number spectroscopic techniques know in the art, such as ATR, DRIFT, specular reflectance or photoacoustic infrared spectroscopic techniques, Raman spectroscopic techniques, UV/Vis spectroscopic techniques, and microwave spectroscopic techniques. Study 1.
  • Oil samples containing 1 to 5,000 ppm of water were prepared by adding a known volume of 50% water in acetone (by volume) to a beaker containing 25 ml of oil. Each mixture was stirred on a magnetic plate for 2 hours to ensure sample homogeneity and to allow acetone evaporation. Oil samples containing >5000 ppm were prepared with more vigorous stirring using an overhead propeller. A known volume of the samples was extracted from the stirred beaker using a micropipette or a 10 ml syringe. Samples were either immediately transferred to a stoppered vessel for measurement by KFT or processed with the membrane.
  • KFT of pure oils and water in oil samples were measured volumetrically on a Metrohm Titrando 841 or coulometically on a Metrohm 756 KFT.
  • HYDRANAL ® - Solver (Crude) oil was used as titration reagent for volumetric titration and HYDRANAL ® - Coelomate AG was used for coulometric KFT.
  • KFT instruments were calibrated using a 1 ml of HYDRANAL ® Water Standard 1%.
  • a stainless-steel membrane assembly (part no.1980-001) obtained from Whatman was modified by removing the outlet tube connector to facilitate transmission of the IR beam through the membrane assembly.
  • IR transparent membranes 13 mm diameter were obtained from Orono Spectral Solutions Inc. Membranes had a thickness of approximately 37 ⁇ m and a measured void fraction of about 55%.
  • Membrane assembly (see Figure 1) consisted of a 13 mm metal screen, followed by the membrane, then two Teflon TM O-rings (13 mm OD, 11 mm ID diameter). The metal screen provided mechanical stability and had 50% throughput across the entire IR spectral region. The two TeflonTM rings provided a seal between the membrane and the top portion of the membrane housing. All spectra were recorded in transmission mode through the LuerTM lock of the assembly mounted at the sample focus of an ABB-Bomem FTLA 2000 FTIR.
  • the membrane remained fully wetted by the oil, to afford transparency in the IR spectral region and to minimize evaporation of the adsorbed water.
  • the membrane assembly was then mounted in a home-built sample holder (see Figure 2) that was cooled to -20 0C.
  • a sample holder that operated at temperatures below 0 0C prevented evaporation of water from the membrane.
  • Recording spectra over 10 second intervals using a standard sample holder, rather than a cooled sample holder, resulted in a decrease in the IR bands due to water with each spectrum.
  • Use of the sample holder pre-cooled to -20 0C resulted in no change in intensity of the water bands for at least 6 minutes, which exceeded the 1-2 minutes used to record an infrared spectrum.
  • the membrane was placed inside the metal assembly and then inserted inside the sample holder that was pre-purged with N2 gas. The openings of the sample holder were covered with parafilm and the assembly placed inside the freezer for 30 minutes. Then the sample holder was mounted in the FTIR sample compartment and an IR spectrum recorded. [0140] All spectra were recorded on an ABB-Bomem FTLA 2000 FTIR equipped with a DTGS detector. A spectrum consisted of 100 coadded interferograms at 8 cm -1 resolution and required about 1 minute to record. A prerecorded reference spectrum was used in all measurements. The reference was recorded through a membrane that was fully wetted with about 5 ⁇ l of the pure oil. Reference spectra were recorded weekly.
  • Transmission IR spectra of all samples were measured for comparative purposes. Spectra were recorded using a 1.2 mm path length transmission liquid cell equipped with CaF 2 windows. A reference spectrum was recorded through an empty transmission cell prior to adding sample. The transmission cell was cleaned between measurements by flushing with acetone, followed by purging with N2 gas. Verification of cleanliness was performed by recording a spectrum through the cell, using an open beam as the reference. The cleaning procedure was repeated until no residual oil or acetone bands were detected in the spectrum.
  • the CCl4 (100 ppm of water) spectrum exhibits two sharp bands at 3707 cm -1 and 3616 cm -1 assigned to the asymmetric and symmetric OH stretching modes of water respectively
  • the power steering fluid spectra exhibit two sharp bands at 3450 cm -1 and 3421 cm -1 , and at higher concentration a broad band near 3400 cm -1 is also observed.
  • the vegetable oil spectra exhibit a series of broad bands over the region of 3700 cm -1 to 3400 cm -1 .
  • the EP fluid spectra lack a significant band near 3400 cm -1 .
  • the variability in the spectra depicted in Figure 3 are indicative of the challenges associated with standard method ASTM E2412 for water measurement and further demonstrate the need for a matrix-specific calibration.
  • the intensity of the band at 3420 cm -1 requires quantification of water via weaker water modes, such as the combination modes at 2174 cm -1 in the IR region or 5185 cm -1 in the near-IR region; an example spectrum is seen in Figure 5(d) for a 1 mL sample of power steering fluid with a 1000 ppm of water.
  • the spectrum shown in Figure 5(d) exhibits narrow regions over the ranges 3100-2800 cm -1 , 1400-1200 cm -1 and 800-600 cm -1 that are opaque due to C-H stretching, bending, and rocking modes, respectively, of the oil.
  • Literature values for the extinction coefficients were used to convert absorbance values of IR bands to ppm levels of water in oil. Agreement with KFT values and those calculated using known extinction coefficients confirms dispersion of liquid water on the membrane, and that the water is devoid of any additives or interferents that would distort the spectrum. Furthermore, slope values of 0.99 and 0.98 for vegetable oil and power steering fluid indicates essentially complete capture of water on the membrane over the entire concentration range. In this example, the slightly decreased slope of 0.95 for EP fluid is attributed to a small fraction of water droplets not captured by the membrane.
  • Total time for sample processing was about 5 minutes per sample, which is significantly faster than the 2 hours per sample needed for volumetric Karl Fischer titration (for samples > 1000 ppm) and on par with the 10 minutes per measurement for coulometric Karl Fischer titration (samples ⁇ 1000 ppm).
  • concentration of water in a sample (C H2O ) in units of ppm is calculated by dividing M H2O by total mass of the sample passed through the membrane. For concentrations at and below 5,000 ppm, water mass is negligible, and total mass of the sample is simply the volume of oil (V) passed through the membrane multiplied by density ( ⁇ ) of the oil.
  • Oil samples containing 1 to 10,000 ppm of water were prepared by adding a known volume of 50% water in acetone (by volume) to a beaker containing 25 ml of oil. Each mixture was stirred on a magnetic plate for 2 hours to ensure sample homogeneity and to allow acetone evaporation. Oil samples containing >5000 ppm of were prepared with more vigorous stirring using an overhead propeller.
  • Calcium oxide was prepared by first grinding with a mortar and pestle to achieve an average diameter of approximately 1.5 ⁇ m as measured by dynamic light scattering on a Malvern Zetasizer. Ground calcium oxide was transferred to a covered crucible and heated in a furnace at 850 °C for two hours to remove residual Ca(OH) 2 and CaCO3.
  • Step A Samples of unknown concentration were analyzed according to a procedure outlined in the flow chart depicted in Figure 7.
  • Step A a sample was tested for water levels in the range of 100 to 1000 ppm.
  • a vial containing 155.5 mg CaO was added quickly (2-3 seconds) to a stirred vial containing 5 ml of oil.
  • the suspension was stirred for 30 minutes to ensure complete reaction of the water with the CaO powder.
  • a 0.4 ml aliquot of the stirred suspension was then drawn into a Luer-LockTM syringe.
  • a plastic 3 x 2 in. card was used to hold the membrane assembly at the sample focus of an ABB Bomem FTLA 2000 FTIR, equipped with a DTGS detector.
  • the card had a 6 mm hole in the center and a plastic male Luer-lockTM connector epoxied to the front of the card and centered over the hole.
  • the female Luer-lockTM of the membrane assembly was mounted to the male Luer-lockTM connector of the sample card and an absorbance spectrum in transmission mode was recorded through the Luer-lockTM.
  • Spectra were recorded using 100 scans (approximately 2 minutes observation time) at a resolution of 8 cm -1 .
  • Reference spectra were recorded with membrane fully wetted with a water free oil sample. While water free reference samples were used presence of water in a reference sample would not interfere with quantification of Ca(OH) 2 band at 3645 cm -1 .
  • Experimental conditions used in Step A, provided in Table 3, were selected to provide a range of 0.12 to 1.2 absorbance units for the band at 3645 cm -1 . This converts to concentrations of water in oil from 100 to 1,000 ppm.
  • a syringe pump operating at 1 ml/min, was used to pass larger volumes through the membrane assembly.
  • the syringe pump was orientated such that the oil passed vertically through the membrane assembly.
  • Table 3 Experimental Parameters used for Step A-D [0161] If the intensity of the band at 3645 cm -1 exceeded a value of 1.2 absorbance after Step A, then the concentration of water exceeded 1,000 ppm. To measure water concentrations between 1,000 to 10,000 ppm, the experimental parameters described for Step D were used (see Table 3). In particular, a 40 ⁇ l sample of the oil was directly deposited onto the membrane using a micropipette. The opening of the disposable micropipette tip was cut to double the size of the tip opening diameter to allow uptake of the particulate suspension.
  • the micropipette was then inserted into a stirred beaker containing the oil sample to extract a 40 ⁇ l aliquot.
  • the top section of the membrane assembly was removed and the 40 ⁇ l was slowly injected onto the surface of the membrane while moving the micropipette tip over the membrane surface to fully wet the membrane with a uniform distribution of CaO powder.
  • the top section of membrane housing was then reattached to the membrane assembly, the membrane assembly attached to the sample card, and an IR spectrum recorded.
  • the amount of CaO added to a water in oil sample was about 10x in excess for concentrations ⁇ 2000 ppm and about 6x in excess for concentrations > 2000 ppm.
  • Ca(OH) 2 was quantified using the intensity (in absorbance units) of the band associated with the OH stretching mode of Ca(OH) 2 at 3645 cm -1 .
  • the amount of Ca(OH) 2 per area of membrane (cl) is calculated according to the Beer’s Law relationship: where ⁇ is the extinction coefficient and A 3645 is the peak absorbance value for the band at 3645 cm -1 .
  • the extinction coefficient ⁇ of 801 cm 2 /g for was determined from the Beer’s Law relationship, using known quantities of Ca(OH) 2 powder pressed in KBr pellets.
  • the total mass of Ca(OH) 2 collected on the membrane ( ) is described by: where Area is the effective area of the membrane.
  • the effective membrane diameter is 11.5 mm, because the TeflonTM O-rings used in the membrane assembly reduce the area of the membrane that the volume of oil is passed through to 1.05 cm 2 .
  • the sample is deposited on the membrane without the TeflonTM O-rings; therefore, the effective area of the membrane is the full area (1.33 cm 2 ).
  • the total mass of Ca(OH) 2 in the beaker is described by: where V is the volume of oil in the beaker and V s is the volume processed through the membrane.
  • Equation 10 is not dependent on the volume of oil in the beaker (V).
  • V volume of oil in the beaker
  • Addition of the same mass of CaO to both beakers would result in twice the amount of Ca(OH) 2 produced in the 10 mL sample, compared to the 5 ml sample.
  • concentration of Ca(OH) 2 in the 10 mL sample is 50% lower, extraction of the same sample volume in the syringe would result in deposition of the same amount of Ca(OH) 2 on the membrane.
  • Infrared spectra depicted in Figure 13 indicate that addition of a stoichiometric amount of CuSO 4 relative to the amount of water in a sample does not result in complete consumption of water; two bands associated with the O-H stretching and bending modes of free water are observed at 3400 and 1640 cm -1 , respectively. In contrast, after addition of 10x excess CuSO 4 , the spectrum obtained exhibited no evidence of water extracted on the membrane (i.e. no bands occurring at 3400 and 1640 cm -1 ), along with an increase in intensity of the band at 1743 cm -1 .
  • Infrared spectra depicted in Figure 14 were obtained after adding CuSO 4 particles to samples containing 10, 100, 500, and 1,000 ppm of water in power steering fluid and then passing known volumes of the suspension through the membrane assembly.
  • the regions between 3000-2800 and 1250-1130 cm -1 are opaque due to the strong C-H modes of the oil and the strong C-F modes of the membrane, respectively.
  • the two bands at 1446 and 1364 cm -1 along with the bands in the 800-600 cm -1 region are due to the C-H bending modes of the power steering fluid.
  • the presence of positive oils bands indicates the presence of more oil in the sample spectrum than in the reference spectrum.
  • the intensity of this band at 1743 cm -1 varies with concentration of water in the oil and volume of sample passed through a membrane. No bands due to the O-H stretching modes of free water near 3400 cm -1 were observed in the spectra. When water is coordinated to the Cu +2 ion in CuSO 4 through the oxygen atom of water, the intensity of the bending mode of water is enhanced relative to the stretching modes.
  • the peak observed at 1743 cm -1 in the spectra of Figure 14 is attributed to the O-H bending vibration mode of CuSO 4 ⁇ H 2 O produced from coordination of a single water molecule to CuSO 4 .

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Abstract

La présente invention concerne des procédés, des kits et des systèmes pour déterminer la teneur en eau d'un échantillon. Dans certains modes de réalisation, les procédés de la présente invention sont destinés à mesurer la concentration d'eau dans des échantillons d'huile.
PCT/US2021/050000 2020-09-14 2021-09-13 Systèmes et procédés pour déterminer la teneur en eau d'un échantillon Ceased WO2022056351A1 (fr)

Priority Applications (3)

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CA3194337A CA3194337A1 (fr) 2020-09-14 2021-09-13 Systemes et procedes pour determiner la teneur en eau d'un echantillon
EP21867736.7A EP4211446A4 (fr) 2020-09-14 2021-09-13 Systèmes et procédés pour déterminer la teneur en eau d'un échantillon
US18/025,938 US20230366814A1 (en) 2020-09-14 2021-09-13 Systems and methods for determining water content in a sample

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US63/078,209 2020-09-14

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WO2025067935A1 (fr) * 2023-09-27 2025-04-03 IFP Energies Nouvelles Analyse de l'eau d'un procédé de séparation en lit mobile simulé par spectroscopie proche infrarouge

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